摘要
目的评定用超高效液相质谱联用(UPLC-MS/MS)法测定比格犬中血浆6-巯基嘌呤(6-MP)的不确定度。方法分析用UPLC-MS/MS测定比格犬血浆6-MP浓度中不确定度的来源并进行合成。结果比格犬血浆中6-MP低浓度(15 ng·mL^(-1))和高浓度(375 ng·mL^(-1))的扩展不确定度分别为1.04 ng·mL^(-1)和30.14 ng·mL^(-1)(P=95%,k=2)。结论UPLC-MS/MS法测定比格犬血浆中6-MP浓度的不确定度,在低浓度时主要由曲线拟合、回收率及基质效应引入,高浓度时主要来源于回收率、曲线拟合和生物样本配置。
Objective To evaluate the uncertainty for the determination of 6-mercaptopurine(6-MP)in beagle dog plasma by UPLC-MS/MS.Methods The whole process during the 6-MP determination was analyzed and the uncertainty from various sources were calculated.The combined and expanded uncertainty were also evaluated.Results The expanded uncertainty of 6-MP at low(15 ng·mL^(-1))and high(375 ng·mL^(-1))levels were 1.04 ng·mL^(-1)and 30.14 ng·mL^(-1),respectively(P=95%,k=2).Conclusion The uncertainty for the determination of 6-MP in beagle dog plasma by UPLCMS/MS at low concentration is mainly caused by calibration curve fitting,recovery and matrix effect,while at high concentration the uncertainty is mainly caused by recovery,calibration curve fitting and sample preparation.
作者
王佳庆
汪祺
史卫忠
张冬婕
宁霄
WANG Jiaqing;WANG Qi;SHI Weizhong;ZHANG Dongjie;NING Xiao(Clinical Trial Center,Beijing Tiantan Hospital,Capital Medical University,Beijing 100050,China;Institute for Control of Chinese Traditional Medicine and Ethnic Medicine,National Institutes for Food and Drug Control,Beijing 100050,China;Department of Pharmacy,Beijing Tiantan Hospital,Capital Medical University,Beijing 100050,China;The Institute for Food and Cosmetics Testing,National Institute of Food and Drug Control,Beijing 100050,China)
出处
《中国药物警戒》
2023年第12期1321-1325,共5页
Chinese Journal of Pharmacovigilance
基金
国家重点研发计划(2021YFC2401100)。
